Electronic Supplementary Information for the manuscript ...



Electronic Supplementary Information for the manuscript submitted to Journal of Materials Chemistry C

Liquid-phase exfoliation of niobium trisulfide and niobium triselenide

Vladimir E. Fedorov,*a, b Sofya B. Artemkina,a Ekaterina D. Grayfer,a Nikolay G. Naumov,a Yuri V. Mironov,a Alexander I. Bulavchenko,a Vladimir I. Zaikovskii,b Irina V. Antonova,c Alexander I. Komonov,c and Maxim V. Medvedevd

aNikolaev Institute of Inorganic Chemistry, Siberian Branch of Russian Academy of Sciences, 3, Acad. Lavrentiev prospect, Novosibirsk, 630090, Russian Federation

bNovosibirsk State University, 2, Pirogova street, Novosibirsk, 630090, Russian Federation

cRzhanov Institute of Semiconductor Physics, Siberian Branch of Russian Academy of Sciences, 13, Acad. Lavrentiev prospect, Novosibirsk, 630090, Russian Federation

dSamsung Advanced Institute of Technology, Suwon, South Korea

*Corresponding author. Tel. +7383-330-92-53; E-mail: fed@niic.nsc.ru

1. Experimental details

The syntheses of niobium trichalcogenides were carried out using high temperature ampoule method starting from high purity elements. Before synthesis the silica ampoule V=16 mL was thoroughly cleaned, dried, heated in vacuum at 800°C to remove traces of absorbed H2O and O2 and cooled under vacuum.

Synthesis of NbS3

The stoichiometric mixture of niobium powder (2.500 g, 0.0269 mol) and sulphur (2.590 g, 0.0809 mol) was loaded into ampoule which was evacuated to 10-5 bar and sealed under dynamic vacuum. The ampoule was heated in electrical furnace as follows: heating to 600°С during 12 h, keeping at 600°С during 120 h, and cooling to room temperature for 5 h. Then the ampoule was cut and the resulting powder was taken out and put under Ar. Yield of NbS3 is quantitative. Powder pattern of NbS3 fits well that calculated for triclinic NbS3 (PDF Number: 71-468, triclinic, Sp. Gr. P-1).

Synthesis of NbSe3

The stoichiometric mixture of niobium powder (3.000 g, 0.0323 mol) and selenium powder (7.650 g, 0.0969 mol) were placed in a quartz vacuum-degassed ampoule and sealed. The ampoule with reaction mixture was heated in a furnace during 6 h to the temperature of 600°С and then kept at this temperature for 74 h. After that the furnace was cooled down to room temperature during 14 h and opened. Yield of NbSe3 is quantitative. XRD powder pattern of the synthesized NbSe3 corresponds to the pattern calculated for monoclinic NbSe3.

2. Uv-vis characterization of dispersions

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Figure S1. Correlation dependence between the concentration of NbS3 / CH3CN dispersion and the value of absorption band at 589 nm.

3. DLS characterization of dispersions

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Figure S2. DLS data for NbS3 colloidal dispersions in 45% EtOH water solution (left); in isopropanol (right).

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Figure S3. DLS data for NbSe3 colloidal dispersion in various solvents

4. AFM characterization of NbS3 samples deposited from acetonitrile dispersion

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Figure S4. Survey AFM image (left) and distribution diagram of upper lengths of the particles NbS3 in acetonitrile colloid solution (right).

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Figure S5. AFM images of small particles in the sample and its profiles.

5. TEM characterization of NbS3 samples deposited from acetonitrile dispersion

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Figure S6. TEM images of NbS3 high-crystalline NbS3 particle (a, b); edges of NbS3 particles (c, d); Figure с shows thin amorphous shell on the surface; NbS3 layer packing (e).

6. Optical images of thin films of NbS3 prepared by filtration and spray method

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Figure S7. Photograph of NbS3 films filtered on Whatman anodisc

(diameter is 25 mm, pores are 0.02 μm

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Figure S8. NbS3 film preparation by spray-method: in process of spraying (left); the resulting NbS3 film (right).

7. XRD characterization of NbS3 films

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Figure S9. Simulation of textured X-Ray diffraction patterns for NbS3 films with variation of empirical coefficient O1.

8. IR spectroscopy data

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Figure S110. IR-spectrum of dispersed NbS3 solid. The band at 568 cm-1 corresponds to S-S bonds, and the band at 400 cm-1 to Nb-S bonds.

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